HRID441558

反应详情

EQUATION

反应方程式

HRID 441558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of trans 3-bromocinnamoyl chloride (12.3 g) in anhydrous toulene (150 ml) was added slowly with stirring to a solution of ethylamine (10 g) in dry ether (100 ml) at room temperature. The reaction mixture was heated at reflux for 1 hour, and the solvent and excess amine were then removed under reduced pressure. The residue was triturated with water, filtered, and recrystallized from ethanol-water to give trans 3-bromo-N-ethylcinnamamide, m.p. 89°-90° C., as a white crystalline material. NMR and IR spectra as well as elemental analysis were consistent with the assigned structure.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 1 hour
  3. customthe solvent and excess amine were then removed under reduced pressure
  4. customThe residue was triturated with water
  5. filtrationfiltered
  6. customrecrystallized from ethanol-water